Triethylamine → N,N-Dimethyl-5-[(1-methyl-1H-imidazol-5-yl)carbonyl]pyridin-2-amine

HRID 627489노트

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HRID 627489 반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:10]2[N:14]([CH3:15])[CH:13]=[N:12][CH:11]=2)=[O:9])=[CH:4][N:3]=1.Cl.[CH3:17][NH:18][CH3:19].CCN(CC)CC>CO>[CH3:17][N:18]([CH3:19])[C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:10]2[N:14]([CH3:15])[CH:13]=[N:12][CH:11]=2)=[O:9])=[CH:4][N:3]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 10473Dimethylamine, hydrochlorideHCID 120166732-Chloro-5-[(1-methyl-1H-imidazol-5-yl)carbonyl]pyridine2회

생성물 1

HCID 86716071N,N-Dimethyl-5-[(1-methyl-1H-imidazol-5-yl)carbonyl]pyridin-2-amine

시약·촉매·용매 1

HCID 887Methanol용매

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온도
75 °C

실험 절차

In a 50-mL round-bottom flask was placed a solution of 2-chloro-5-[(1-methyl-1H-imidazol-5-yl)carbonyl]pyridine (250 mg, 1.13 mmol, Intermediate 22, step c), dimethylamine hydrochloride (96 mg, 1.2 mmol), and Et3N (342 mg, 3.39 mmol) in methanol (15 mL). The resulting mixture was heated at 75° C. overnight and concentrated under vacuum. The residue was purified by flash column chromatography (silica gel column, 100:0-20:1 CH2Cl2/MeOH) to give the title compound as a light yellow solid.

후처리

  1. customIn a 50-mL round-bottom flask was placed
  2. concentrationconcentrated under vacuum
  3. customThe residue was purified by flash column chromatography (silica gel column, 100:0-20:1 CH2Cl2/MeOH)

출처 및 근거

ORD 기록
ord-e7ec708e8e7440d5af384e792da973a2
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09309222B2

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